Thiourea → 5-(Pyrimid-5-ylmethyl)-2-thiouracil

HRID 2228915노트

반응식

HRID 2228915 반응식
[Na].[NH2:2][C:3]([NH2:5])=[S:4].[CH:6]([CH:8]([CH2:14][C:15]1[CH:16]=[N:17][CH:18]=[N:19][CH:20]=1)[C:9](OCC)=O)=[O:7]>C(O)C>[N:17]1[CH:16]=[C:15]([CH2:14][C:8]2[C:6](=[O:7])[NH:2][C:3](=[S:4])[NH:5][CH:9]=2)[CH:20]=[N:19][CH:18]=1

참가 물질

5

반응물 3

HCID 2723790ThioureaHCID 5360545SodiumHCID 21936283Ethyl 2-formyl-3-(5-pyrimidyl)propionate

생성물 1

HCID 109660395-(Pyrimid-5-ylmethyl)-2-thiouracil수율 33.7%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

Sodium (0.25 g) was dissolved in ethanol (5 ml), thiourea (0.77 g) added, and the mixture stirred under reflux for 1 hour. A solution of ethyl 2-formyl-3-(5-pyrimidyl)propionate (1.99 g) in ethanol (5 ml) was added slowly, and reflux continued for 18 hours. The solvent was evaporated, and the residue taken up in water and washed with dichloromethane. The aqueous solution was acidified to pH 5, and the precipitate filtered off, washed with water and dried to obtain 5-(pyrimid-5-ylmethyl)-2-thiouracil (0.71 g). 1H-NMR (d6-DMSO) δ 3.58 (2H, s), 7.54 (1H, s), 8.70 (2H, s) and 9.02 (1H, s). MPt 265-6° C.

후처리

  1. temperatureunder reflux for 1 hour
  2. temperaturereflux
  3. customThe solvent was evaporated
  4. washwashed with dichloromethane
  5. filtrationthe precipitate filtered off
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-c8e9c08581ba4f549f1968c14b1f0d59
출처 데이터셋
uspto-grants-2002_07
특허 번호
US06417192B1

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